CN101916619B - Nano particle doped REBCO film and preparation method thereof - Google Patents
Nano particle doped REBCO film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nano particle doped REBCO film and a preparation method thereof, and belongs to the technical field of high-temperature superconducting material preparation. The film consists of an REBCO film and nano particles dispersed in the REBCO. The preparation method comprises the following steps of: preparing 1.0 to 2.0 mol/L of REBCO precursor solution, adding inorganic salt of Sn, Zr, Ta or Nb into the precursor solution and then coating the solution to a single crystal substrate, pre-sintering the substrate in wet oxygen of less than 400 DEG C, then sintering the obtained precursor amorphous film for 1 to 4 hours at the temperature of between 800 and 850 DEG C, introducing wet Ar/O2 mixed gas into the precursor amorphous film in front 3/4 time, introducing dry Ar/O2 mixed gas into the precursor amorphous film in later 1/4 time, switching the dry Ar/O2 mixed gas to pure oxygen when the temperature is reduced to 500 DEG C, preserving the heat for 2 to 4 hours, and cooling the film along with a furnace. The doped REBCO film has higher superconducting performance under a high-temperature high field and application prospect.
Description
Technical field
The invention belongs to the high temperature superconducting materia preparing technical field, being specifically related to rare earth is the technology of preparing of barium-copper oxide superconductive high temperature superconducting thin film.
Background technology
Since have high irreversible, high current capacity, low A.C. losses, potential price advantage is that the barium-copper oxide high-temperature superconductor just has been subjected to paying close attention to widely since being found the end of the eighties in last century always based on the rare earth of YBCO.High-temperature superconductor is considered to be widely used in aspects such as cable, generator, nulcear magnetic resonance (NMR), and the application of these aspects not only requires superconductor to have stronger conductive capability under null field, more requires to have good conductive capability under externally-applied magnetic field.
With YBCO is that example is come, because the critical current density (J of ybco film under externally-applied magnetic field
c) value decline rapidly along with the increase of externally-applied magnetic field, must be by artificially introduce some nano level defectives suppress ybco film as pinning center J at ybco film
cThe reduction of value.At present, efficient ways is exactly that second particle introducing nano level non-superconducting in the ybco film the inside suppresses externally-applied magnetic field to ybco film J as pinning center the most
cThe influence of value.From present research, research is introduced nano-particle doped ybco film and is mainly concentrated on pulsed laser deposition technique (PLD), but it is also very weak to adopt chemical solution technology (as the MOD method) to prepare the research of nano-particle doped ybco film.The MOD method is as a kind of with low cost and be applicable to the method for extensive generation, and itself just has broad application prospects; With respect to the PLD technology, it is simple to adopt the MOD method to prepare nano-particle doped ybco film method, and the accurately raw material and the ratio thereof of controlled doping.In addition, adopting the MOD method to prepare the selected doped raw material of nano-particle doped ybco film at present all is organic slaine, and its price is comparatively expensive.Select for use the relatively low inorganic salts of cost to have application prospect more as doped raw material.
Summary of the invention
The objective of the invention is to solve prior art problems, provide a kind of chemical solution method that adopts to prepare nano-particle doped REBCO film and preparation method thereof.This method equipment is simple, with low cost, is suitable for large-scale industrial production.
A kind of nano-particle doped REBCO film provided by the present invention, mainly by the REBCO film be scattered in the REBCO film in second mutually nano particle form, the amount of substance of nano particle is 1%～10% of REBCO, wherein the REBCO film refers to the barium-copper oxide high-temperature superconducting thin film of rare earth system, as YBCO, GdBCO, YbBCO etc.; The second phase nano particle mainly refers to the nano particle of the material of perovskite structure, as barium zirconate (BZO), barium stannate (BSO) etc.
The present invention adopts MOD chemical method with low cost to prepare nano-particle doped REBCO film, the precursor aqueous solution of the REBCO that at first to mix, again through filming, low temperature and high temperature sintering obtain nano-particle doped REBCO film, concrete steps are as follows:
1) preparation of REBCO precursor aqueous solution:
Is to be dissolved in deionized water at 1: 2: 3 lanthanon acetate, barium acetate and Schweinfurt green according to the ratio of amount of substance, adds and Cu again
2+The amount of substance ratio of ion is behind 1: 2.3～2.5 the trifluoroacetic acid, to react 2～4 hours in 50～60 ℃ of water-baths; Obtain blue transparent colloidal liquid 50～60 ℃ of following evaporation and concentration at last,, obtain the REBCO precursor aqueous solution of 1.0-2.0mol/L with the methyl alcohol dilution;
The inorganic salts (chloride or nitrate) that add a certain amount of Sn, Zr, Ta or Nb toward the REBCO precursor aqueous solution are as doped raw material, the abundant REBCO precursor aqueous solution that obtains mixing after the dissolving, and the consumption of inorganic salts is 1～10% of a REBCO amount of substance; Wherein, Sn and Zr salt can directly add in the precursor aqueous solution, and the inorganic salts of Ta and Nb need be dissolved in the absolute methanol earlier, and then add in the precursor aqueous solution;
2) coating of film: the mode of REBCO precursor aqueous solution by spin coating or dip-coating be coated to obtain precursor film on the single crystal substrates;
3) low temperature presintering: the pre-burning in being lower than 400 ℃ wet oxygen of coated precursor film is obtained forerunner's amorphous film, sintering process is as follows: the programming rate of room temperature to 200 ℃ is 135 ℃/hour, programming rate between 200 ℃-250 ℃ is 3-7 ℃/hour, programming rate between 250 ℃-300 ℃ is 30 ℃/hour, and the programming rate between 300 ℃-400 ℃ is 300 ℃/hour;
4) high temperature sintering: in 800-850 ℃ of following sintering 1-4 hour, in the sintering process, in preceding 3/4 time period, feeding oxygen content was the wet Ar/O of 100-1000ppm with forerunner's amorphous film
2Gaseous mixture, in 1/4 time period of back, feeding oxygen content is the dried Ar/O of 100-1000ppm
2It is the dried Ar/O of 100-1000ppm continuing to feed oxygen content that gaseous mixture, sintering finish the back
2Gaseous mixture is cooling down, changes purity oxygen when temperature drops to 500 ℃ into, and is incubated 2-4 hour, obtains nano-particle doped REBCO film with the stove cooling.
Wherein, step 2) adopt the spin coating mode that the REBCO precursor aqueous solution is coated in lanthanum aluminate (LAO) or strontium titanates (STO) substrate in, the revolution of filming is 3000-6000 rev/min, and the time of filming is 1-2 minute; When adopting the mode of dip-coating, the pull rate of filming is the 5-80 mm/min;
Wet oxygen described in the step 3) is to realize that by the container that distilled water is housed that oxygen is fed water-bath heating bath temperature is 20-50 ℃, oxygen flow be the 0.2-1.0 liter/minute, the temperature range that feeds wet oxygen is between 150～400 ℃;
Wet Ar/O described in the step 4)
2Gaseous mixture is by with Ar/O
2Gaseous mixture feeds that the container that distilled water is housed of water-bath heating realizes, bath temperature is 30-50 ℃, mixed gas flow be the 0.2-1.5 liter/minute.
Compared with prior art, the present invention has following beneficial effect:
1) ybco film that mixes with respect to MOD preparation at present commonly used, doped raw material provided by the present invention is inorganic salts, cost is cheap relatively, and can to use at the rare earth based on YBCO widely be in the barium-copper oxide high temperature superconducting materia, to improve the critical current density of such superconducting thin film under magnetic field.Under uniform temp, magnetic field is high more, the J of doped samples
cBe higher than pure ybco film more.The REBCO film that the present invention mixes has higher superconductivity under the high temperature High-Field, comparing pure ybco film more has application prospect.
2) the invention provides employing MOD method and prepared the nano particles that are suitable for doped YBCO more, expanded the application of nano-particle doped ybco film.
Description of drawings
The XRD figure of gained film among Fig. 1: the embodiment 1;
The J of gained film among Fig. 2: the embodiment 1
cCurve (77K) with changes of magnetic field;
The XRD figure of gained film among Fig. 3: the embodiment 2;
The J of gained film among Fig. 4: the embodiment 2
cCurve (77K) with changes of magnetic field;
The XRD figure of gained film among Fig. 5: the embodiment 3;
The J of gained film among Fig. 6: the embodiment 3
cCurve (77K) with changes of magnetic field;
The surface topography of prepared film among Fig. 7: the embodiment 4;
The T of prepared film among Fig. 8: the embodiment 5
cValue.
Below in conjunction with the drawings and the specific embodiments the present invention is described in further details.
Embodiment
1) 0.01mol acetic acid yttrium, 0.02mol barium acetate and 0.03mol Schweinfurt green are dissolved in the deionized water, add adding and Cu more again
2+The amount of substance ratio of ion is behind 1: 2.3 the trifluoroacetic acid, and reaction is 3 hours in 50 ℃ of water-baths; Obtain blue transparent colloidal liquid 50 ℃ of following evaporation and concentration at last,, obtain the YBCO precursor aqueous solution of 1.5mol/L with the methyl alcohol dilution; The SnCl that adds 0.0006mol in the YBCO precursor aqueous solution for preparing
4, after treating fully to dissolve, the YBCO precursor aqueous solution that obtains mixing;
2) adopt spin coating method that the YBCO precursor aqueous solution is coated in the LAO substrate and obtain wet film, the revolution of filming is 4000 rev/mins, and the time of filming is 1 minute;
3) wet film low temperature presintering in the wet oxygen below 400 ℃ is obtained forerunner's amorphous film, wherein, the programming rate of room temperature to 200 ℃ is 135 ℃/hour, programming rate between 200 ℃-250 ℃ is 3.5 ℃/hour, programming rate between 250 ℃-300 ℃ is 30 ℃/hour, and the programming rate between 300 ℃-400 ℃ is 300 ℃/hour; Wet oxygen is that the container that distilled water is housed of the water-bath heating of 30 ℃ of oxygen feedings is realized that since 150 ℃ of feedings, oxygen flow is 0.2 liter/minute;
4) forerunner's amorphous film is incubated 2 hours down at 820 ℃, wherein, the wet Ar/O of feeding in preceding 1.5 hours
2(oxygen content is 200ppm to gaseous mixture, with Ar/O
2The container that distilled water is housed of the water-bath heating that the gaseous mixture feeding is 50 ℃ realizes that mixed gas flow is 0.5 liter/minute), Ar/O is done in feeding in back 0.5 hour
2Gaseous mixture after sintering finishes, is continuing to feed dried Ar/O
2Lower the temperature under the condition of gaseous mixture, when temperature drops to 500 ℃, change purity oxygen into, and be incubated 2 hours, then with stove cooling, the ybco film that obtains mixing.
The XRD result of this film in the drawings except that the diffraction maximum of substrate, only shows (00l) diffraction maximum of YBCO as shown in Figure 1, illustrates that this film has good face and is orientated outward, and barium stannate does not embody in the drawings because content is less; The J of the ybco film that shown in Figure 2 is pure YBCO and Sn element (barium stannate) mixes
cVariation relation with externally-applied magnetic field.As seen, the Jc value of the ybco film of Sn element (barium stannate) doping is significantly improved under externally-applied magnetic field.
1) 0.005mol gadolinium acetate, 0.01mol barium acetate and 0.015mol Schweinfurt green are dissolved in the deionized water, add adding and Cu more again
2+The amount of substance ratio of ion is behind 1: 2.4 the trifluoroacetic acid, and reaction is 3 hours in 50 ℃ of water-baths; Obtain blue transparent colloidal liquid 50 ℃ of following evaporation and concentration at last,, obtain the GdBCO precursor aqueous solution of 1.5mol/L with the methyl alcohol dilution; The SnCl that adds 0.0003mol in the GdBCO precursor aqueous solution for preparing
4, after treating fully to dissolve, the GdBCO precursor aqueous solution that obtains mixing;
2) adopt spin coating method that the GdBCO precursor aqueous solution that mixes is coated in the LAO substrate and obtain wet film, the revolution of filming is 4000 rev/mins, films 2 minutes time;
3) wet film low temperature presintering in the wet oxygen below 400 ℃ is obtained forerunner's amorphous film, identical among concrete sintering process and the embodiment 1;
4) forerunner's amorphous film is incubated 2.0 hours down at 850 ℃, wherein, the wet Ar/O of feeding in preceding 1.5 hours
2(oxygen content is 500ppm to gaseous mixture, with Ar/O
2The container that distilled water is housed of the water-bath heating that the gaseous mixture feeding is 50 ℃ realizes that mixed gas flow is 0.35 liter/minute), Ar/O is done in feeding in back 0.5 hour
2Gaseous mixture after sintering finishes, is continuing to feed dried Ar/O
2Lower the temperature under the condition of gaseous mixture, when temperature drops to 500 ℃, change purity oxygen into, and be incubated 4 hours, then with stove cooling, the GdBCO film that obtains mixing.
The XRD of this film as shown in Figure 3, the visible GdBCO film that mixes has the good c-axis orientation, can not be subjected to the mixing influence of particle of its orientation.In addition, the Sn that can also find to mix from the XRD is with BaSnO
3The form of particle exists.Compare the J under its externally-applied magnetic field with pure GdBCO
cValue is improved, as shown in Figure 4.
1) 0.0025mol acetic acid ytterbium, 0.0025mol acetic acid yttrium, 0.01mol barium acetate and 0.015mol Schweinfurt green are dissolved in the deionized water, add adding and Cu more again
2+The amount of substance ratio of ion is behind 1: 2.3 the trifluoroacetic acid, and reaction is 3 hours in 50 ℃ of water-baths; Obtain blue transparent colloidal liquid 50 ℃ of following evaporation and concentration at last,, obtain the Yb of 1.5mol/L with the methyl alcohol dilution
0.5Y
0.5The BCO precursor aqueous solution; TaCl with 0.0003mol
5Be dissolved in the absolute methanol, after treating fully to dissolve, add Yb to
0.5Y
0.5In the BCO precursor aqueous solution, the Yb that obtains mixing
0.5Y
0.5The BCO precursor aqueous solution;
2) adopt spin coating method with the Yb that mixes
0.5Y
0.5The BCO precursor aqueous solution is coated in the STO substrate and obtains wet film, and the revolution of filming is 4500 rev/mins, and the time of filming is 2 minutes;
3) sintering process is identical with the step 3) of embodiment 1;
4) sintering process is identical with the step 4) of embodiment 1;
The XRD of this film as shown in Figure 5, the visible Yb that mixes
0.5Y
0.5The BCO film has good c-axis orientation, can not be subjected to the mixing influence of particle of its orientation.Compare present embodiment Ta element (barium tantalate) doping Yb with pure YBCO
0.5Y
0.5J under the BCO film externally-applied magnetic field
cValue is improved, as shown in Figure 6.
1) 0.01mol acetic acid yttrium, 0.02mol barium acetate and 0.03mol Schweinfurt green are dissolved in the deionized water, add adding and Cu more again
2+The amount of substance ratio of ion is behind 1: 2.4 the trifluoroacetic acid, and reaction is 2.5 hours in 50 ℃ of water-baths; Obtain blue transparent colloidal liquid 50 ℃ of following evaporation and concentration at last,, obtain the YBCO precursor aqueous solution of 1.2mol/L with the methyl alcohol dilution; NbCl with 0.0006mol
5Be dissolved in the absolute methanol, after treating fully to dissolve, add in the YBCO precursor aqueous solution YBCO precursor aqueous solution that obtains mixing to;
2) adopt dip-coating method that the YBCO precursor aqueous solution that mixes is coated in the LAO substrate and obtain wet film, pull rate is 20 mm/min;
3) wet film low temperature presintering in oxygen wet below 400 ℃ is obtained forerunner's amorphous film, wherein, the programming rate between 200 ℃-250 ℃ is 5 ℃/hour, and all the other conditions are all identical with embodiment 1;
4) forerunner's amorphous film is incubated 2 hours down at 840 ℃, wherein, the wet Ar/O of feeding in preceding 1.5 hours
2(oxygen content is 200ppm to gaseous mixture, with Ar/O
2The container that distilled water is housed of the water-bath heating that the gaseous mixture feeding is 50 ℃ realizes that mixed gas flow is 0.5 liter/minute), Ar/O is done in feeding in back 0.5 hour
2Gaseous mixture after sintering finishes, is continuing to feed dried Ar/O
2Lower the temperature under the condition of gaseous mixture, when temperature drops to 500 ℃, change purity oxygen into, and be incubated 2 hours, then with stove cooling, the ybco film that obtains mixing.
The surface topography of this film as shown in Figure 7, as seen, film surperficial dense, and have very tiny particle.
1) 0.01mol acetic acid yttrium, 0.02mol barium acetate and 0.03mol Schweinfurt green are dissolved in the deionized water, add adding and Cu more again
2+The amount of substance ratio of ion is behind 1: 2.4 the trifluoroacetic acid, and reaction is 3 hours in 50 ℃ of water-baths; Obtain blue transparent colloidal liquid 50 ℃ of following evaporation and concentration at last,, obtain the YBCO precursor aqueous solution of 1.5mol/L with the methyl alcohol dilution; Zr (NO with 0.0006mol
3)
4Add in the YBCO precursor aqueous solution, after treating fully to dissolve, the YBCO precursor aqueous solution that obtains mixing;
2) adopt dip-coating method that the YBCO precursor aqueous solution that mixes is coated in the LAO substrate and obtain wet film, pull rate is 50 mm/min;
3) wet film low temperature presintering in wet oxygen below 400 ℃ is obtained forerunner's amorphous film, wherein, the programming rate between 200 ℃-250 ℃ is 5 ℃/hour, and all the other conditions are all identical with embodiment 1;
4) forerunner's amorphous film is incubated 2.5 hours down at 820 ℃, wherein, the wet Ar/O of feeding in preceding 2 hours
2(oxygen content is 500ppm to gaseous mixture, with Ar/O
2The container that distilled water is housed of the water-bath heating that the gaseous mixture feeding is 50 ℃ realizes that mixed gas flow is 0.8 liter/minute), Ar/O is done in feeding in back 0.5 hour
2Gaseous mixture after sintering finishes, is continuing to feed dried Ar/O
2Lower the temperature under the condition of gaseous mixture, when temperature drops to 500 ℃, change purity oxygen into, and be incubated 2 hours, then with stove cooling, the ybco film that obtains mixing.
The critical transition temperature of this film is about 90K, and width of transition is 0.5K, as shown in Figure 8.
Claims (4)
1. the preparation method of a nano-particle doped REBCO film is characterized in that, may further comprise the steps:
1) preparation of REBCO precursor aqueous solution
Is to be dissolved in deionized water at 1: 2: 3 lanthanon acetate, barium acetate and Schweinfurt green according to the ratio of amount of substance, adds and Cu again
2+The amount of substance ratio of ion is behind 1: 2.3～2.5 the trifluoroacetic acid, to react 2～4 hours in 50～60 ℃ of water-baths; Obtain blue transparent colloidal liquid 50～60 ℃ of following evaporation and concentration at last,, obtain the REBCO precursor aqueous solution of 1.0-2.0mol/L with the methyl alcohol dilution;
The inorganic salts that add a certain amount of Sn, Zr, Ta or Nb toward the REBCO precursor aqueous solution are as doped raw material, the abundant REBCO precursor aqueous solution that obtains mixing after the dissolving, and the consumption of inorganic salts is 1～10% of a REBCO amount of substance; Wherein, Sn and Zr salt directly add in the precursor aqueous solution, and the inorganic salts of Ta and Nb need be dissolved in the absolute methanol earlier, and then add in the precursor aqueous solution;
2) coating of film: the mode of REBCO precursor aqueous solution by spin coating or dip-coating be coated to obtain precursor film on the single crystal substrates;
3) low temperature presintering: the pre-burning in being lower than 400 ℃ wet oxygen of coated precursor film is obtained forerunner's amorphous film, sintering process is as follows: the programming rate of room temperature to 200 ℃ is 135 ℃/hour, programming rate between 200 ℃-250 ℃ is 3-7 ℃/hour, programming rate between 250 ℃-300 ℃ is 30 ℃/hour, and the programming rate between 300 ℃-400 ℃ is 300 ℃/hour;
4) high temperature sintering: in 800-850 ℃ of following sintering 1-4 hour, in the sintering process, in preceding 3/4 time period, feeding oxygen content was the wet Ar/O of 100-1000ppm with forerunner's amorphous film
2Gaseous mixture, in 1/4 time period of back, feeding oxygen content is the dried Ar/O of 100-1000ppm
2It is the dried Ar/O of 100-1000ppm continuing to feed oxygen content that gaseous mixture, sintering finish the back
2Gaseous mixture is cooling down, changes purity oxygen when temperature drops to 500 ℃ into, and is incubated 2-4 hour, obtains nano-particle doped REBCO film with the stove cooling.
2. the preparation method of a kind of nano-particle doped REBCO film of claim 1, it is characterized in that, step 2) adopt the spin coating mode that the REBCO precursor aqueous solution is coated in lanthanum aluminate (LAO) or strontium titanates (STO) substrate in, the revolution of filming is 3000-6000 rev/min, and the time of filming is 1-2 minute; When adopting the mode of dip-coating, the pull rate of filming is the 5-80 mm/min.
3. the preparation method of a kind of nano-particle doped REBCO film of claim 1, it is characterized in that, wet oxygen described in the step 3) is to realize by the container that distilled water is housed that oxygen is fed the water-bath heating, bath temperature is 20-50 ℃, oxygen flow be the 0.2-1.0 liter/minute, the temperature range that feeds wet oxygen is between 150～400 ℃.
4. the preparation method of a kind of nano-particle doped REBCO film of claim 3 is characterized in that, the wet Ar/O described in the step 4)
2Gaseous mixture is by with Ar/O
2Gaseous mixture feeds that the container that distilled water is housed of water-bath heating realizes, bath temperature is 30-50 ℃, mixed gas flow be the 0.2-1.5 liter/minute.
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| CN102424575A (en) * | 2011-09-13 | 2012-04-25 | 西南交通大学 | Preparation method of Co-doped GdBCO superconducting film |
| CN102412017B (en) * | 2011-10-19 | 2014-06-04 | 中国科学院电工研究所 | Method for improving upper critical field and critical current density of iron-based superconductor |
| CN103102162A (en) * | 2013-01-30 | 2013-05-15 | 江苏天诚线缆集团有限公司 | Method for preparing element doping yttrium, gadolinium, barium, copper and oxygen high-temperature superconducting film |
| CN103274681A (en) * | 2013-03-28 | 2013-09-04 | 北京工业大学 | Nb-doped YxYb1-xBCO superconductive film and preparation method thereof |
| CN103274682B (en) * | 2013-05-11 | 2014-10-15 | 中国科学院电工研究所 | Preparation method of high-temperature superconductive film |
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